1-Methylpiperazine → HCID 12733914、化合物

HRID 544222ノート

反応式

HRID 544222 の反応式
[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([Cl:14])=[C:10](Cl)[CH:11]=2)[C:6](=[O:15])[C:5]([C:16]([OH:18])=[O:17])=[CH:4]1)[CH3:2].[CH3:19][N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1>O>[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([Cl:14])=[C:10]([N:23]3[CH2:24][CH2:25][N:20]([CH3:19])[CH2:21][CH2:22]3)[CH:11]=2)[C:6](=[O:15])[C:5]([C:16]([OH:18])=[O:17])=[CH:4]1)[CH3:2]

参加物

4

反応物 2

HCID 531671-MethylpiperazineHCID 127338866,7-Dichloro-1-ethyl-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

生成物 1

HCID 12733914HCID 12733914、化合物収率 30%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 1-ethyl-6,7-dichloro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid 2.86 g (0.01 mole), N-methylpiperazine 10 g (0.1 mole) and 15 ml water was heated in a sealed tube at 125°-130° C. (inner temperature) for 19 hours. After cooling, the reaction mixture was evaporated under vacuum and acidified with acetic acid. Insoluble matters were filtered off and the filtrate was neutralized with an aqueous solutiong of NaOH to pH 7, extracted with CHCl3, dried with anhydrous Na2SO4, and the solvent was distilled off. The residue was recrystallized from a mixed solvent of CHCl3 and benzene to give 1.05 g (30%) of 1-ethyl-6-chloro-7-(4-methyl-1-piperazinyl)-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid. Colorless needles.

後処理

  1. temperaturewas heated in a sealed tube at 125°-130° C. (inner temperature) for 19 hours
  2. temperatureAfter cooling
  3. customthe reaction mixture was evaporated under vacuum
  4. filtrationInsoluble matters were filtered off
  5. extractionextracted with CHCl3
  6. dry with materialdried with anhydrous Na2SO4
  7. distillationthe solvent was distilled off
  8. customThe residue was recrystallized from a mixed solvent of CHCl3 and benzene

出典と根拠

ORDレコード
ord-acaa4dd7379e47b2a113b4193cc44c09
出典データセット
uspto-grants-1984_05
特許番号
US04448962

反応ノート

読み込み中…